CN104961146A - Nanometer sheet aluminum hydroxide gel and preparation method thereof - Google Patents
Nanometer sheet aluminum hydroxide gel and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nanometer sheet aluminum hydroxide gel and a preparation method thereof, and belongs to the technical field of IIIA-class hydroxide nanometer material preparation. The nanometer sheet aluminum hydroxide gel is nanometer sheet gel with high specific surface area, wherein the nanometer sheet gel is formed by trivalent aluminum hydroxide Al(OH)3 and all stages of dehydration products Al2O3.x(H2O). The method includes the steps of directly putting absolute methanol and anhydrous aluminum chloride in a reaction still to conduct reaction to form a colorless transparent solution, sealing the reaction still and keeping the reaction still at a temperature of 220 DEG C to 300 DEG C for one hour, and naturally cooling to the room temperature to obtain the nanometer sheet aluminum hydroxide gel. The nanometer sheet aluminum hydroxide gel has the advantages of being large in specific surface area, small in thickness and the like, and the preparation method is easy, feasible, high in repeatability, low in cost and free of pH value adjustment or vacuum environment.
Description
Technical field
The invention belongs to technical field prepared by IIIA race Nano material of hydrate, particularly a kind of method preparing nano-sheet alumine hydroxide colloid simply, efficiently.
Background technology
Nano material broadly refers to the general name of the hyperfine material having at least one dimension to be in nano-scale range in three dimensions or to be made up of as basic structural unit the material in this range scale.Due to the small-size effect of nanoparticle, surface effects, quantum size effect and macro quanta tunnel effect etc. make they magnetic, optical, electrical, responsive etc. in present the feature that conventional material do not possess.Therefore nanoparticle has broad application prospects in the sintering, catalysis, sensing, ceramic toughening etc. of magneticsubstance, electronic material, optical material, high compactedness material.
Nano aluminum hydroxide gel body, aluminum oxyhydroxide nanometer colloid, aluminium oxide nano colloid are widely used in the industries such as electrician, electric wire, cable, material of construction, plastics and rubber item in life.And the aluminium hydroxide inorganic fire-retarded additive that to be consumption in life maximum and most widely used, be widely used in the industries such as thermosetting material, thermoplastic material, synthetic rubber, coating and building materials.Aluminium base oxyhydroxide, oxyhydroxide multifunctional material is at environment, the energy, medical treatment, the fields such as national defense safety have important potential application, colloidal aluminium hydroxide is that a class has micro-pore, high-specific surface area, the multifunctional material of high specific strength, can be used as sorbent material, siccative or catalyzer, in petrochemical complex, weaving, the fields such as oxygen have potential application, existing alumine hydroxide colloid material is mainly with block, micron particles and powder are main, limit it further to apply, alumine hydroxide colloid material with specific small size and morphology controllable and preparation method thereof, become present physical, one of study hotspot of chemistry and material science, and the alumine hydroxide colloid material of high-specific surface area has irreplaceable advantage in the Application Areas of the concrete pattern of ask for something.
And prepare in the method for alumine hydroxide colloid existing, most methods is tended to use promoting agent, precipitation agent, dispergator etc. to prepare aluminium hydroxide.In experimentation, also want control ph, step is complicated, and program is loaded down with trivial details, and production cost is higher, and the reaction times is also longer, limits production and the application of aluminium hydroxide isocolloid.
Summary of the invention
The technical problem to be solved in the present invention is, nano-sheet alumine hydroxide colloid providing a kind of high-specific surface area and preparation method thereof.
Technical problem of the present invention solves by following technical scheme:
A kind of nano-sheet alumine hydroxide colloid, it is characterized in that, be by the oxyhydroxide Al (OH) of trivalent aluminium
3and dewatered product Al at different levels
2o
3x (H
2o) the nano flake gel formed, wherein 1 < x≤3, the thickness of nano flake is 3 ~ 20nm.
The thickness preferably 3 ~ 10nm of described nano flake.
A kind of preparation method of nano-sheet alumine hydroxide colloid, it is characterized in that, colourless transparent solution is formed after anhydrous methanol and Aluminum chloride anhydrous are directly put into reaction kettle for reaction, then reactor is sealed and be incubated 1 hour at 220 DEG C ~ 300 DEG C, naturally cool to room temperature, namely obtain nano-sheet alumine hydroxide colloid; The usage ratio of anhydrous methanol and Aluminum chloride anhydrous is that every gram of Aluminum chloride anhydrous uses 40 milliliters of anhydrous methanols.
Described insulation carries out better effects if in 1 hour at 280 ~ 300 DEG C.
Alumine hydroxide colloid of the present invention, the oxyhydroxide Al (OH) of general reference aluminium
3and the amorphous gel-like product that dewatered product at different levels is formed, macroscopically present from low to high by water white transparency particulate state to white powder by preparation temperature; From microcosmic, these colloids have assembles by nano flake the multilevel hierarchy formed, and when temperature of reaction is 240 DEG C, sample is piled up layer by layer by a large amount of nano-sheets, formed one irregular, the sheet aggregate of undefined structure.When temperature of reaction is 260 DEG C, sample is formed by the curling accumulation of a large amount of nano flakes, forms microspheroidal and the block sheet aggregate coexisted.When temperature of reaction is 280 DEG C, sample is piled up layer by layer by a large amount of nano flakes, formed one rough, microspheric sheet aggregate.When temperature of reaction is 300 DEG C, sample forms by being similar to spherical Nano microsphere gathering in a large number.Nano microsphere is interconnected to form microsphere aggregation body, and each Nano microsphere is in layer wrapped up by nano flake, forms Nano microsphere shape.When temperature of reaction is 280 ~ 300 DEG C, the thickness of the nano flake of acquisition is less than 10nm, the thinlyyest reaches 3 ~ 4nm.
Beneficial effect:
For aluminum hydroxide material, the present invention obtains nano-sheet alumine hydroxide colloid first, the thinnest 3nm that reaches of thickness, compared to published nano-aluminum hydroxide colloid, sample of the present invention has controlled sheet-like morphology and higher specific surface area, has special important, irreplaceable effect in the Application Areas of the concrete pattern of ask for something.Preparation method disclosed in this invention overcomes the many restrictions in preparation method in the past, devise a kind of method preparing nano-sheet alumine hydroxide colloid, the method is simple, reproducible, with low cost, without the need to adjust ph, without the need to vacuum environment, the abundance of the nano aluminum hydroxide gel body prepared, purity is high.
Accompanying drawing explanation
Fig. 1 is the sample figure of the nano-sheet alumine hydroxide colloid that example 1 obtains.
Fig. 2 is the SEM figure of the nano-sheet alumine hydroxide colloid that example 1 obtains.
Fig. 3 is the SEM figure of the nano-sheet alumine hydroxide colloid that example 1 obtains.
Fig. 4 is the TEM figure of the nano-sheet alumine hydroxide colloid that example 1 obtains.
Fig. 5 is the XRD figure of the nano-sheet alumine hydroxide colloid that example 1 obtains.
Fig. 6 is the sample figure of the nano-sheet alumine hydroxide colloid that example 2 obtains.
Fig. 7 is the SEM figure of the nano-sheet alumine hydroxide colloid that example 2 obtains.
Fig. 8 is the TEM figure of the nano-sheet alumine hydroxide colloid that example 2 obtains.
Fig. 9 is the XRD figure of the nano-sheet alumine hydroxide colloid that example 2 obtains.
Figure 10 is the sample figure of the nano-sheet alumine hydroxide colloid that example 3 obtains.
Figure 11 is the SEM figure of the nano-sheet alumine hydroxide colloid that example 3 obtains.
Figure 12 is the TEM figure of the nano-sheet alumine hydroxide colloid that example 3 obtains.
Figure 13 is the XRD figure of the nano-sheet alumine hydroxide colloid that example 3 obtains.
Figure 14 is the sample figure of the nano-sheet alumine hydroxide colloid that example 4 obtains.
Figure 15 is the SEM figure of the nano-sheet alumine hydroxide colloid that example 4 obtains.
Figure 16 is the TEM figure of the nano-sheet alumine hydroxide colloid that example 4 obtains.
Figure 17 is the XRD figure of the nano-sheet alumine hydroxide colloid that example 4 obtains.
Figure 18 is the sample figure of the nano-sheet alumine hydroxide colloid that example 5 obtains.
Figure 19 is the SEM figure of the nano-sheet alumine hydroxide colloid that example 5 obtains.
Figure 20 is the TEM figure of the nano-sheet alumine hydroxide colloid that example 5 obtains.
Figure 21 is the XRD figure of the nano-sheet alumine hydroxide colloid that example 5 obtains.
Figure 22 is the sample figure of the methylate of the Al that example 6 obtains.
Figure 23 is the SEM figure of the methylate of the Al that example 6 obtains.
Figure 24 is the TEM figure of the methylate of the Al that example 6 obtains.
Figure 25 is the XRD figure of the methylate of the Al that example 6 obtains.
Embodiment
Embodiment 1 prepares the whole process of nano-sheet alumine hydroxide colloid at 300 DEG C
First 8ml anhydrous methanol is got by graduated cylinder correct amount, weigh the Aluminum chloride anhydrous getting 0.2g again in the balance, the anhydrous methanol of the 0.2g Aluminum chloride anhydrous weighed up and 8ml is directly put into the tetrafluoroethylene reactor that volume is 10ml, at room temperature there is vigorous reaction in Aluminum chloride anhydrous and anhydrous methanol, finally at room temperature form transparent colourless solution, with irritating smell.Stove is put in reactor sealing, at 300 DEG C, is incubated 1 hour.After it reacts completely, reactor is taken out, makes it naturally cool to room temperature.Finally obtain white powder aluminium hydrate nano material.
Fig. 1 provides nano-sheet alumine hydroxide colloid sample picture prepared by above-mentioned condition.Can find out and prepare nano-sheet alumine hydroxide colloid at 300 DEG C, after naturally cooling to room temperature, finally obtain white powder aluminium hydrate nano material.As can be seen from the SEM figure of Fig. 2, form by being similar to spherical Nano microsphere gathering in a large number at the nano-sheet alumine hydroxide colloid of 300 DEG C of preparations.Nano microsphere is interconnected to form microsphere aggregation body.By magnification, as can be seen from Figure 3, each Nano microsphere is in layer wrapped up by nano flake, forms Nano microsphere shape.Fig. 4 provides the TEM figure of nano-sheet alumine hydroxide colloid prepared by above-mentioned condition.From then on TEM figure can obviously find out temperature of reaction at 300 DEG C time the nano-sheet alumine hydroxide colloid that obtains be the Nano microsphere that nano flake that size is very little is gathered into, thickness is the thinnest reaches 3 ~ 4nm for it.Fig. 5 provides the XRD figure that above-mentioned condition prepares nano-sheet alumine hydroxide colloid.Can find out interval to there is a stronger diffraction zone at 15 ° to 30 °, and occur without obvious peak crystallization.Prove that the sample this temperature is obtained becomes colloidality better.
Embodiment 2 prepares the whole process of nano-sheet alumine hydroxide colloid at 280 DEG C
8ml anhydrous methanol is got by graduated cylinder correct amount, weigh the Aluminum chloride anhydrous getting 0.2g again in the balance, the anhydrous methanol of the 0.2g Aluminum chloride anhydrous weighed up and 8ml is directly put into the tetrafluoroethylene reactor that volume is 10ml, at room temperature there is vigorous reaction in Aluminum chloride anhydrous and anhydrous methanol, finally at room temperature form transparent colourless solution, with irritating smell.Stove is put in reactor sealing, and 280 DEG C are incubated 1 hour.After it reacts completely, reactor is taken out, makes it naturally cool to room temperature.Finally obtain white powder aluminium hydrate nano material
Fig. 6 provides nano-sheet alumine hydroxide colloid sample picture prepared by above-mentioned condition.Can find out that the nano aluminum hydroxide gel body 280 DEG C of preparations finally obtains the nano material of white powder aluminium hydroxide after naturally cooling to room temperature; As can be seen from the SEM figure of Fig. 7, piled up layer by layer by a large amount of nano flakes at the nano-sheet alumine hydroxide colloid of 280 DEG C of preparations, formed one rough, microspheric sheet aggregate, Fig. 8 provide nano-sheet alumine hydroxide colloid prepared by above-mentioned condition TEM figure.From then on TEM figure can obviously find out temperature of reaction at 280 DEG C time the nano-sheet alumine hydroxide colloid that obtains be still the Nano microsphere that the very little nano flake of size is gathered into, its thickness is less than 10nm.Fig. 9 provides the XRD figure of nano-sheet alumine hydroxide colloid prepared by above-mentioned condition.
Embodiment 3 prepares the whole process of nano-sheet alumine hydroxide colloid at 260 DEG C
8ml anhydrous methanol is got by graduated cylinder correct amount, weigh the Aluminum chloride anhydrous getting 0.2g again in the balance, the anhydrous methanol of the 0.2g Aluminum chloride anhydrous weighed up and 8ml is directly put into the tetrafluoroethylene reactor that volume is 10ml, at room temperature there is vigorous reaction in Aluminum chloride anhydrous and anhydrous methanol, finally at room temperature form transparent colourless solution, with irritating smell.Stove is put in reactor sealing, and 260 DEG C are incubated 1 hour.After it reacts completely, reactor is taken out, makes it naturally cool to room temperature.Finally obtain white powder aluminium hydrate nano material.
Figure 10 provides nano-sheet alumine hydroxide colloid sample picture prepared by above-mentioned condition.Can find out that the nano-sheet alumine hydroxide colloid 260 DEG C of preparations finally obtains the nano material of white powder aluminium hydroxide after naturally cooling to room temperature; As can be seen from the SEM figure of Figure 11, formed by the curling accumulation of a large amount of nano flakes at the nano-sheet alumine hydroxide colloid of 260 DEG C of preparations, form microspheroidal and the block sheet polymer coexisted, Figure 12 provides the TEM figure of nano-sheet alumine hydroxide colloid prepared by above-mentioned condition.From then on TEM figure can find out that the nano-sheet alumine hydroxide colloid size obtained when temperature of reaction is 260 DEG C obviously increases.Figure 13 provides the XRD figure of above-mentioned condition nano-sheet alumine hydroxide colloid.
Embodiment 4 prepares the whole process of nano-sheet alumine hydroxide colloid at 240 DEG C
8ml anhydrous methanol is got by graduated cylinder correct amount, weigh the Aluminum chloride anhydrous getting 0.2g again in the balance, the anhydrous methanol of the 0.2g Aluminum chloride anhydrous weighed up and 8ml is directly put into the tetrafluoroethylene reactor that volume is 10ml, at room temperature there is vigorous reaction in Aluminum chloride anhydrous and anhydrous methanol, finally at room temperature form transparent colourless solution, with irritating smell.Stove is put in reactor sealing, and 240 DEG C are incubated 1 hour.After it reacts completely, reactor is taken out, makes it naturally cool to room temperature.Finally obtain white powder aluminium hydrate nano material.
Figure 14 provides nano-sheet alumine hydroxide colloid sample picture prepared by above-mentioned condition.Can find out that the nano-sheet alumine hydroxide colloid 240 DEG C of preparations finally obtains the nano material of white powder aluminium hydroxide after naturally cooling to room temperature; As can be seen from the SEM figure of Figure 15,240 DEG C preparation nano-sheet alumine hydroxide colloids by a large amount of nano flakes pile up layer by layer form one irregular, the sheet aggregate of undefined structure, Figure 16 provides the TEM figure of nano-sheet alumine hydroxide colloid prepared by above-mentioned condition.Figure 17 provides the XRD figure of nano-sheet alumine hydroxide colloid prepared by above-mentioned condition.
Embodiment 5 prepares the whole process of nano-sheet alumine hydroxide colloid at 220 DEG C
8ml anhydrous methanol is got by graduated cylinder correct amount, weigh the Aluminum chloride anhydrous getting 0.2g again in the balance, the anhydrous methanol of the 0.2g Aluminum chloride anhydrous weighed up and 8ml is directly put into the tetrafluoroethylene reactor that volume is 10ml, at room temperature there is vigorous reaction in Aluminum chloride anhydrous and anhydrous methanol, finally at room temperature form transparent colourless solution, with irritating smell.Stove is put in reactor sealing, and 220 DEG C are incubated 1 hour.After it reacts completely, reactor is taken out, makes it naturally cool to room temperature.Finally obtain that quality is comparatively hard, water white transparency particulate state aluminium hydrate nano material.
Figure 18 provides nano-sheet alumine hydroxide colloid sample picture prepared by above-mentioned condition.Can find out after naturally cooling to room temperature, finally obtain at the nano-sheet alumine hydroxide colloid of 220 DEG C of preparations that quality is comparatively hard, the nano material of water white transparency particulate state aluminium hydroxide.Nano-aluminum hydroxide colloid sample obtained at this point in the reaction has significant difference with example above.As can be seen from the SEM figure of Figure 19, piled up at the nano-sheet alumine hydroxide colloid of 220 DEG C of preparations the sheet aggregate forming layer by layer by a large amount of nano flakes, Figure 20 provides the TEM figure of nano aluminum hydroxide gel body prepared by above-mentioned condition.Figure 21 provides the XRD figure of nano-sheet alumine hydroxide colloid prepared by above-mentioned condition.
Example 6 prepares the whole process of the methylate of aluminium at 200 DEG C
This example is counter-example, illustrates when temperature of reaction is lower than 220 DEG C, and the product that reaction generates is not nano-sheet alumine hydroxide colloid, but the methylate of aluminium
8ml anhydrous methanol is got by graduated cylinder correct amount, weigh the Aluminum chloride anhydrous getting 0.2g again in the balance, the anhydrous methanol of the 0.2g Aluminum chloride anhydrous weighed up and 8ml is directly put into the tetrafluoroethylene reactor that volume is 10ml, at room temperature there is vigorous reaction in Aluminum chloride anhydrous and anhydrous methanol, finally at room temperature form transparent colourless solution, with irritating smell.Stove is put in reactor sealing, and 200 DEG C are incubated 1 hour.After it reacts completely, reactor is taken out, makes it naturally cool to room temperature, obtain white milky solution, put into stink cupboard ventilation and dry, finally obtain harder, the water white crystalline material of quality.
Figure 22 provides the methylate picture in kind of aluminium prepared by above-mentioned condition.Can find out the methylate of preparing aluminium at 180 DEG C ventilate dry after finally obtain that quality is comparatively hard, the crystalline material of white clear, as can be seen from the SEM figure of Figure 23, piled up at the methylate of the aluminium of 200 DEG C of preparations the sheet aggregate forming layer by layer by a large amount of nano flakes, Figure 24 provides the TEM figure of the methylate of aluminium prepared by above-mentioned condition.Figure 25 provides the XRD figure of the methylate of aluminium prepared by above-mentioned condition, can find out when temperature of reaction is 200 DEG C, the XRD figure of products therefrom there occurs considerable change, diffraction zone intensity corresponding in the XRD spectrum of sample is lower, but near 56 °, there is strong and sharp diffraction peak, prove that product is not now nano-sheet alumine hydroxide colloid, but the methylate of aluminium.
Claims (4)
1. a nano-sheet alumine hydroxide colloid, is characterized in that, is by the oxyhydroxide Al (OH) of trivalent aluminium
3and dewatered product Al at different levels
2o
3x (H
2o) the nano flake gel formed, wherein 1 < x≤3, the thickness of nano flake is 3 ~ 20nm.
2. a kind of nano-sheet alumine hydroxide colloid according to claim 1, is characterized in that, the thickness of described nano flake is 3 ~ 10nm.
3. the preparation method of the nano-sheet alumine hydroxide colloid of a claim 1, it is characterized in that, colourless transparent solution is formed after anhydrous methanol and Aluminum chloride anhydrous are directly put into reaction kettle for reaction, then reactor is sealed and be incubated 1 hour at 220 DEG C ~ 300 DEG C, naturally cool to room temperature, namely obtain nano-sheet alumine hydroxide colloid; The usage ratio of anhydrous methanol and Aluminum chloride anhydrous is that every gram of Aluminum chloride anhydrous uses 40 milliliters of anhydrous methanols.
4. the preparation method of a kind of nano-sheet alumine hydroxide colloid according to claim 3, is characterized in that, described insulation is carried out for 1 hour at 280 ~ 300 DEG C.
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| CN1608997A (en) * | 2004-10-27 | 2005-04-27 | 上海大学 | Prepn process of nano aluminium hydroxide |
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